Simultaneous determination of sildenafil and its active metabolite UK-103,320 in human plasma using liquid chromatography-tandem mass spectrometry

Simultaneous determination of sildenafil and its active metabolite UK-103,320 in human plasma using liquid chromatography-tandem mass spectrometry
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DOI:
10.1016/s0731-7085(03)00088-8
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发表时间:
2003-06-01
影响因子:
3.4
通讯作者:
Lee, HS
Lee, HS
中科院分区:
医学3区
文献类型:
--
作者:
Kim, J;Ji, HY;Lee, HS

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建立了同时测定人血浆中西地那非及其活性N-去甲基代谢物UK-103,320的液相色谱-串联质谱法。在碱性pH值下,用二氯甲烷从人血浆中提取西地那非(UK-103,320)和内标物(DA-8159)。在Luna苯基己基柱上以乙腈-甲酸铵(10 mM,pH 6.0)(60:40,v/v)混合物作为移动的流动相进行反相LC分离。分析物的检测采用电喷雾串联质谱法在多反应监测模式下进行。西地那非和UK-103,320的定量下限为2.0 ng/ml。该方法具有良好的灵敏度、精密度、准确度、回收率和选择性。(C)2003 Elsevier Science B. V.保留所有权利。
A liquid chromatography-tandem mass spectrometric method for the simultaneous determination of sildenafil and its active N-demethylated metabolite, UK-103,320 in human plasma was developed. Sildenafil, UK-103,320 and the internal standard (DA-8159) were extracted from human plasma with dichloromethane at basic pH. A reverse-phase LC separation was performed on Luna phenylhexyl column with the mixture of acetonitrile-ammonium formate (10 mM, pH 6.0) (60:40, v/v) as mobile phase. The detection of analytes was performed using an electrospray ionization tandem mass spectrometry in the multiple reaction-monitoring mode. The lower limits of quantification for sildenafil and UK-103,320 were 2.0 ng/ml. The method showed a satisfactory sensitivity, precision, accuracy, recovery and selectivity. (C) 2003 Elsevier Science B.V. All rights reserved.